Month: May 2021

Electric Literature of 444-29-1, A common heterocyclic compound, 444-29-1, name is 1-Iodo-2-(trifluoromethyl)benzene, molecular formula is C7H4F3I, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

General procedure: A Schlenk tube was charged with MCM-41-Sb,Py-CuI (122mg, 0.05mmol), triphenyphosphine (26mg, 0.10mmol), and K2CO3 (276mg, 2.0mmol). The tube was evacuated and backfilled with argon. Then, aryl halide (1.0mmol), terminal alkyne (1.2mmol) and DMF (4mL) were added under argon. The tube was sealed, and the reaction mixture was stirred at 100C for 6-24h. The reaction mixture was cooled to room temperature, diluted with ethyl acetate (20mL), and filtered. The MCM-41-Sb,Py-CuI complex was washed with distilled water (2×5mL), DMF (2×5mL), and ethanol (2×5mL) and reused in the next run. The filtrate was washed with water, dried over MgSO4 and concentrated under reduced pressure. The residue was purified by flash column chromatography on silica gel (petroleum/ethyl acetate=30:1-60:1) to provide the desired product.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Related Products of 4949-69-3, These common heterocyclic compound, 4949-69-3, name is 4-Iodo-3-methylaniline, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

3-Thiophenecarboxylic acid (2.0 g, 15.6 mmol) was dissolved in methylene chloride (100 rnL) and 2 drops of DMF were added. The mixture was cooled to about 0 0C and oxalyl chloride (1.5 mL, 17.1 mmol) was added slowly and allowed to warm to room temperature. Gas evolution was observed during warming. 3-Methyl-4-iodoaniline (5.45 g, 23.5 mmol), 4 drops of pyridine and K2CO3 (2.58 g, 18.7 mmol) are dissolved in CH2Cl2 (10 mL) and cooled to about 0 0C. After about Ih, the acid chloride mixture is slowly added to the cooled aniline mixture and allowed to warm to room temperature and stirred for about 18h. The resulting mixture is filtered, washed with ethyl acetate and the filtrate is concentrated to a brown oil. The crude material was purified via flash chromatography (10-30% ethyl acetate in hexanes) to afford the desired product (1.56 g, 29%) as an off-white solid.

The synthetic route of 4949-69-3 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 6828-35-9, name is 5-Chloro-2-iodoaniline, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 6828-35-9, Recommanded Product: 6828-35-9

To a round-bottomed flask charged with 5-chloro-2-iodoaniline (1 g, 3.95 mmol, 1 equiv) was added a solution of 1:1 pyridine in CH2Cl2 (0.7 M, 40 mL) and the reaction mixture was cooled to 0 C. 4-Methylbenzenesulfonyl chloride (750 mg, 3.95 mmol, 1 equiv) was added portionwise, and the reaction mixture was allowed to slowly warm to room temperature and then stirred for 24 h. Upon completion of the reaction, water (80 mL) and CH2Cl2 (80 mL) were added. The reaction mixture was separated and the organics were washed with 1 N NaOH (2 × 40 mL), 1 N HCl (2×40 mL), and brine (2 × 40 mL). The organics were then passed through a hydrophobic frit and concentrated under reduced pressure to give a crude residue, which was purified by flash chromatography (silica gel, 0-12% EtOAc in petroleum ether) to afford the title compound as an off white solid (890 mg, 52%).1H NMR (CDCl3, 500 MHz): delta 7.72-7.65 (m, 3H), 7.57 (d, J = 8.5 Hz, 1H), 7.27 (d, J = 8.0 Hz, 2H), 6.88-6.80 (m, 2H), 2.42 (s, 3H).13C NMR (CDCl3, 126 MHz): delta 144.1, 139.1, 138.1, 135.1, 135.1, 129.4, 127.0, 126.4, 121.4, 88.3, 21.2. Characterisation data is consistent with literature reported values.4

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 5-Chloro-2-iodoaniline, other downstream synthetic routes, hurry up and to see.

Adding a certain compound to certain chemical reactions, such as: 61272-76-2, name is 4-Fluoro-2-iodoaniline, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 61272-76-2, name: 4-Fluoro-2-iodoaniline

General procedure: A mixture of 2-iodoaniline (0.5 mmol), isothiocyanate (0.6 mmol), CuO nanoparticles (0.05 mmol), and Cs2CO3 (1.5 mmol) in PEG-400 (3mL) was stirred at 80°C for 8h (Scheme 1). After the reaction, the reaction mixture was centrifuged and catalyst was separated from the reaction mixture and then followed by washing with ethyl acetate and acetone, dried in vacuo and used directly for further catalytic reactions. The cooled solution was partitioned between ethyl acetate and water, and the organic layer was washed with water and brine, and then dried over Na2SO4. After the removal of the solvent in vacuo, the residue was purified by silica-gel chromatography to give the desired N-substituted-2-aminobenzothiazoles. All the compounds were characterized by comparison with authentic samples [41].

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Fluoro-2-iodoaniline, and friends who are interested can also refer to it.

Electric Literature of 90347-66-3, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 90347-66-3, name is Methyl 3-iodo-4-methylbenzoate, This compound has unique chemical properties. The synthetic route is as follows.

A suspension of 4-methylimidazole (1, 3.0 g, 36 mmol), 2 (4.8 g, 20 mmol), K2CO3(4.5 g, 33 mmol), CuI (1.14 g, 6 mmol) and 8-hydroxyquinoline (0.56 g, 4 mmol) in DMSO(20 mL) was heated at 120 C overnight under nitrogen. After cooling, water was added andthe mixture was extracted with EtOAc twice. The combined organic layers were washed withbrine, dried over Na2SO4 and concentrated. The residue was purified by silica gel columnchromatography to give 3 (2.8 g, 58%) as a yellow solid. LCMS (m/z: m+1): 242.2. A mixtureof 4 (7.26 g, 26.3 mmol), 5 (3.0 g, 17.5 mmol), K2CO3 (4.84 g, 35.0 mmol), DMEDA (386 mg,4.38 mmol) and CuI (834 mg, 0.871 mmol) in 90 ml of dioxane was stirred at 100 C under N2for 18h. The mixture was filtered, concentrated and purified by column chromatography to give6 (2.2 g, 39%) as a slightly yellow solid. LCMS (m/z: m+1): 320.2. To a solution of 6 (2.2 g,6.89 mmol) in THF/water (60/30 mL) was added LiOH (496 mg, 20.7 mmol). The reactionwas stirred at room temperature overnight, concentrated. To the residue water (30 ml) wasadded and then acidified to pH 4 with aqueous KHSO4. The precipitate was filtered and washedwith water and EtOAc. The cake was collected and dried to give 7 (1.4 g, 67%) as a whitesolid. LCMS: m/z: (M+1): 306. To a solution of 7 (100 mg, 0.33 mmol) in NMP (2 mL) wasadded SOCl2 (58 mg, 0.49 mmol). The reaction was heated at 90 C for 1 hour before 3 (80mg, 0.33 mmol) was added. The resulting mixture was stirred at 90 C for 3 hours. The reactionwas quenched with water and basified with aqueous NaOH. The mixture was extracted withEtOAc twice. The combined organic layers were washed with brine, dried over Na2SO4 andconcentrated. The residue was purified by reverse prep-HPLC and then silica gel prep-TLC togive 1a (22 mg, 13%) as a white solid.

The chemical industry reduces the impact on the environment during synthesis Methyl 3-iodo-4-methylbenzoate. I believe this compound will play a more active role in future production and life.

Electric Literature of 689260-53-5, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 689260-53-5 name is 2-Bromo-5-iodo-1,3-dimethylbenzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

To 2-Bromo-5-iodo-1,3-Dimethylbenzene(300 mg, 0.965 mmol),1-Amino cyclopropanecarboxylic acid(195 mg, 1.93 mmol),A mixture of copper (I) iodide (37 mg, 0.194 mmol) and diazabicycloundecene (0.50 ml, 3.35 mmol) in dimethylacetamide (2.6 ml) was heated at 120 C for 3 hours under a nitrogen stream Stirring. The reaction mixture was purified by silica gel column chromatography (Wakosil C18, acetonitrile-water (0.1% formic acid)1 – ((4-Bromo-3,5-Dimethylphenyl)Amino)Cyclopropanecarboxylic acid(219 mg, 80%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Bromo-5-iodo-1,3-dimethylbenzene, and friends who are interested can also refer to it.

Electric Literature of 61203-48-3,Some common heterocyclic compound, 61203-48-3, name is 2-Iodo-4,5-dimethoxybenzoic acid, molecular formula is C9H9IO4, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

General procedure: NaIO4 (6.7 g, 31 mmol, 1.0 equiv) and2-iodobenzoic acid (7.4 g, 30 mmol, 1.0 equiv) were suspended in 30% (v:v) aqueousacetic acid (45 mL). The reaction mixture was vigorously stirred and refluxed for 3 hprotecting from light. Cold water (120 mL) was then added and allowed to cool toroom temperature. After 1 h, the crude product was collected by filtration, washedwith ice water (3 x 30 mL) and acetone (3 x 30 mL). After air-drying in the dark,hydroxybenziodoxole 2 was yielded as a white solid.

The synthetic route of 61203-48-3 has been constantly updated, and we look forward to future research findings.

Related Products of 83863-33-6,Some common heterocyclic compound, 83863-33-6, name is 5-Iodo-2-methylaniline, molecular formula is C7H8IN, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

solution of 5-iodo-2-methyl-phenylamine (20.4 g, 87.6 mmol) in 200 mL of dry CH2Cl2 was cooled to 0 C and acetic anhydride (16.5 mL, 175 mmol) was added dropwise. The mixture was heated to 50 C for 2 h and then cooled to 22 C. The resulting white precipitate was filtered to give c (18.4 g, 76%): MS m/z = 276 (M+H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Iodo-2-methylaniline, its application will become more common.

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 3268-21-1, name is 1,4-Diiodo-2,3,5,6-tetramethylbenzene, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 1,4-Diiodo-2,3,5,6-tetramethylbenzene

1,4-Diiodo-2,3,5,6-tetramethylbenzene (1.16 g, 3 mmol),5-(tributyltin)-2,2′-bithiophene (5.6 g, 12 mmol) obtained in Example 1,Pd(PPh3)4 (24.3 mg, 0.021 mmol) was added sequentially under a nitrogen atmosphere.Add 25 ml of DMF (N,N-dimethylformamide),Rapidly warmed to 130 C, the system refluxed for 16 h,The reaction was shut down, cooled to room temperature, extracted with deionized water and dichloromethane respectively. The obtained organic phase was dried over anhydrous MgSO 4 and then purified by column chromatography. The stationary phase was 300 mesh silica gel and the mobile phase was dichloromethane. / petroleum ether (1:5), collecting the eluent containing the target product to evaporate the solvent,Obtaining 1.04 g of a yellow solid benzene-methyl-dithiophene derivative in a yield of 90%

According to the analysis of related databases, 3268-21-1, the application of this compound in the production field has become more and more popular.

Some common heterocyclic compound, 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene, molecular formula is C8H3F6I, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. HPLC of Formula: C8H3F6I

General procedure: Arene (0.10 mmol, 1.0 equiv), Pd(OAc)2 (2.2 mg, 10 mumol,10 molpercent), ligand (15 molpercent or 20 molpercent), hydrogen phosphate (15 molpercent for benzylamine substrate), aryl iodide (0.3 mmol, 3.0 equiv.) and silver acetate (50 mg, 0.30 mmol, 3.0 equiv.) were added into a 2-dram reaction vial. Solvent and (+)-NBE-CO2Me (20 molpercent or 50 molpercent) were added to the mixture. The vial was flushed with N2 and capped. The reaction mixture was then stirred at the selected temperature for 12?24 h. After cooling to room temperature, the mixture was filtered through Celite and eluted with ethyl acetate. The filtrate was evaporated under reduced pressure. Purification by preparative thin-layer chromatography afforded the desired product.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 328-73-4, its application will become more common.